CN114544832A - Method for rapidly detecting azo dye in textile - Google Patents
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- CN114544832A CN114544832A CN202210164635.XA CN202210164635A CN114544832A CN 114544832 A CN114544832 A CN 114544832A CN 202210164635 A CN202210164635 A CN 202210164635A CN 114544832 A CN114544832 A CN 114544832A
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- 239000004753 textile Substances 0.000 title claims abstract description 40
- 239000000987 azo dye Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 25
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000010828 elution Methods 0.000 claims abstract description 14
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 238000001291 vacuum drying Methods 0.000 claims abstract description 12
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Natural products OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 9
- JDWPDZLCSRBZPY-SQGDDOFFSA-N C(=O)(O)C(C(=O)O)N[C@@H](C)C(=O)O.[Na].[Na].[Na] Chemical compound C(=O)(O)C(C(=O)O)N[C@@H](C)C(=O)O.[Na].[Na].[Na] JDWPDZLCSRBZPY-SQGDDOFFSA-N 0.000 claims abstract description 9
- CIWBSHSKHKDKBQ-DUZGATOHSA-N D-isoascorbic acid Chemical compound OC[C@@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-DUZGATOHSA-N 0.000 claims abstract description 9
- 235000010350 erythorbic acid Nutrition 0.000 claims abstract description 9
- 229940026239 isoascorbic acid Drugs 0.000 claims abstract description 9
- XEHNLVMHWYPNEQ-UHFFFAOYSA-N 2,3-dihydro-1h-inden-2-amine;hydron;chloride Chemical compound Cl.C1=CC=C2CC(N)CC2=C1 XEHNLVMHWYPNEQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- JRMAQQQTXDJDNC-UHFFFAOYSA-M 2-ethoxy-2-oxoacetate Chemical compound CCOC(=O)C([O-])=O JRMAQQQTXDJDNC-UHFFFAOYSA-M 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 19
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical group CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 12
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 239000012071 phase Substances 0.000 claims description 9
- 239000007790 solid phase Substances 0.000 claims description 8
- JVVXZOOGOGPDRZ-SLFFLAALSA-N [(1R,4aS,10aR)-1,4a-dimethyl-7-propan-2-yl-2,3,4,9,10,10a-hexahydrophenanthren-1-yl]methanamine Chemical compound NC[C@]1(C)CCC[C@]2(C)C3=CC=C(C(C)C)C=C3CC[C@H]21 JVVXZOOGOGPDRZ-SLFFLAALSA-N 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000002137 ultrasound extraction Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 5
- XKCQASMZNPBLKI-UHFFFAOYSA-N phosphorosooxymethane Chemical compound COP=O XKCQASMZNPBLKI-UHFFFAOYSA-N 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 4
- 230000003247 decreasing effect Effects 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 125000004494 ethyl ester group Chemical group 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 239000004318 erythorbic acid Substances 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 abstract description 2
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 2
- 150000004982 aromatic amines Chemical class 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 229960001484 edetic acid Drugs 0.000 description 9
- 230000000711 cancerogenic effect Effects 0.000 description 8
- 231100000315 carcinogenic Toxicity 0.000 description 8
- 238000004043 dyeing Methods 0.000 description 5
- 238000007639 printing Methods 0.000 description 4
- 229920002994 synthetic fiber Polymers 0.000 description 3
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 229930182817 methionine Natural products 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 231100000915 pathological change Toxicity 0.000 description 2
- 230000036285 pathological change Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 206010005003 Bladder cancer Diseases 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 208000023915 Ureteral Neoplasms Diseases 0.000 description 1
- 206010046392 Ureteric cancer Diseases 0.000 description 1
- 208000007097 Urinary Bladder Neoplasms Diseases 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 231100000405 induce cancer Toxicity 0.000 description 1
- 230000003211 malignant effect Effects 0.000 description 1
- 208000020984 malignant renal pelvis neoplasm Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 231100000175 potential carcinogenicity Toxicity 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 201000007444 renal pelvis carcinoma Diseases 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000979 synthetic dye Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 201000011294 ureter cancer Diseases 0.000 description 1
- 201000005112 urinary bladder cancer Diseases 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for rapidly detecting azo dyes in textiles. In the technical scheme, firstly, a material to be detected with certain fineness is mixed with ethylenediamine tetraacetic acid and diethyl ether, so that an extraction system of a composite component is constructed, and azo dyes are fully dissolved out under the action of the extraction system; on the basis, the invention adopts a centrifugation and layering method to separate extraction phases, and further utilizes a low-temperature vacuum drying means to extract the component to be detected. In addition, the isoascorbic acid and 2-aminoindan hydrochloride are added before detection to play a role in protection, and a composite system to be detected is further constructed by utilizing the components of the ethyl oxalate, the dicarboxymethylalanine trisodium and the like. On the basis of the technical scheme, the invention performs detection through HPLC, and obtains a detection result by specific chromatographic conditions and an elution method. The invention has the advantages of simple operation, high detection speed, high accuracy, outstanding technical advantages and good popularization prospect.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to a method for rapidly detecting azo dyes in textiles.
Background
Azo dyes are organic compounds with aryl groups connected with two ends of azo groups, are synthetic dyes which are most widely applied to textile and clothing in printing and dyeing processes, are used for dyeing and printing various natural and synthetic fibers, and are also used for coloring paint, plastics, rubber and the like. Under special conditions, it can decompose to produce more than 20 carcinogenic aromatic amines, and through activation, it changes the DNA structure of human body to cause pathological changes and induce cancer.
Azo dyes have a wide spectrum of colors including red, orange, yellow, blue, violet, black, etc., and are of complete color types, good color and certain fastness. Therefore, the dye is widely applied to dyeing and printing of various natural and synthetic fibers and is also used for coloring paint, plastics, rubber and the like. And is also a synthetic material of textile garments most used in the printing and dyeing process. The carcinogenicity problem is that the aromatic amine which can be reduced in some azo dyes has potential carcinogenicity to human body or animal through long-term research and clinical test. In the long-term contact of the textile and the skin, part of azo dyes on the textile can be transferred to the skin of a person under certain special conditions, particularly poor dyeing fastness, form harmful components which are absorbed by the skin and diffused in the human body, and then the harmful components are mixed with substances released in the normal metabolism process of the human body to generate reduction reaction, so that the DNA structure of the human body is changed, pathological changes are caused, malignant tumor substances are induced, and malignant diseases such as bladder cancer, ureter cancer, renal pelvis cancer and the like are caused.
Azo dyes are not carcinogenic per se, and up to 3000 azo dyes are currently used, wherein most of the azo dyes are safe, and only a small part of the azo dyes which can reduce and release the specified twenty-more aromatic amines is forbidden, and about 200 azo dyes are forbidden.
In general, the forbidden aromatic amines in the textile may come from additives such as adhesives, auxiliaries and the like besides dyes. There are three possible routes to carcinogenic aromatic amines in the production process: 1. the raw materials are carried with carcinogenic aromatic amine, like the form of isomer; 2. carcinogenic aromatic amine is used as raw material. The conversion of most coupling reactions is not quantitative, so that these carcinogenic aromatic amines are entrained in the final product; 3. azo dyes, which consist of carcinogenic aromatic amines as diazo component, may be affected by the external environment during use, releasing these carcinogenic aromatic amines. For the reasons, the determination of the azo dye content is an important link for detecting the quality of the textile. In the prior art, the conventional detection method generally has the defects of complex operation, low accuracy and the like, and is not beneficial to ensuring the detection efficiency of products.
Disclosure of Invention
The invention aims to provide a method for rapidly detecting azo dyes in textiles aiming at the technical defects of the prior art so as to solve the technical problems of complex operation and low accuracy of the conventional detection method.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for rapidly detecting azo dyes in textiles comprises the following steps:
1) crushing the textile to be detected by using a homogenizer, mixing the crushed textile with ethylenediamine tetraacetic acid, uniformly mixing the crushed textile with the ethylenediamine tetraacetic acid, adding diethyl ether, mixing and centrifuging the mixture until the liquid is layered, and transferring the lower liquid phase into another container;
2) drying the other container in vacuum drying equipment, taking the residual solid phase, adding an isoascorbic acid aqueous solution into the residual solid phase, repeatedly blowing and absorbing until redissolving, adding dehydroabietylamine acetic acid, heating to 75 ℃, and keeping for 20 min;
3) adding the ethyl oxalate, the 3-methylphosphinic acid and the trisodium dicarboxymethylalanine into the product obtained in the step 2), performing vortex mixing assisted ultrasonic extraction, adding 2-aminoindan hydrochloride into the product, and filtering the product through a filter membrane with the aperture of 0.22 mu m to obtain a substance to be detected;
4) detecting the substance to be detected obtained in the step 3) under the following chromatographic conditions: the chromatographic column is a C18 column; the detector is VWD; the mobile phase A is methanol, and the mobile phase B is isooctane; gradient elution; in the first 8min of gradient elution, the volume fraction of methanol is reduced from 80% to 30%, and the volume fraction of isooctane is increased from 20% to 70%; and in the 8 th-20 th min of gradient elution, the volume fraction of methanol is increased from 30% to 80%, and the volume fraction of isooctane is decreased from 70% to 20%.
Preferably, the particle size of the textile to be detected after the pulverization in the step 1) is not more than 1 mm.
Preferably, the molar ratio of the ethylenediamine tetraacetic acid to the diethyl ether in the step 1) is 1: 5.
Preferably, in step 1), during said transfer, the temperature does not exceed 8 ℃.
Preferably, the temperature of vacuum drying in the step 2) is not higher than 65 ℃, and the time of vacuum drying is not more than 40 min.
Preferably, the concentration of the aqueous solution of erythorbic acid in the step 2) is 0.8 mol/L.
Preferably, the final concentration of dehydroabietylamine acetic acid in step 2) is 0.6 mol/L.
Preferably, the molar ratio of the ethyl ester of the methionine, the 3-methylphosphonite propionic acid and the trisodium dicarboxymethylalanine in the step 3) is 1: 2: 3.6.
Preferably, the time length of the vortex mixing auxiliary ultrasonic extraction in the step 3) is 80-120 min.
Preferably, in step 3), the material to be filtered is heated to 55 ℃ before passing through a 0.22 μm pore size filter.
The invention provides a method for rapidly detecting azo dyes in textiles. In the technical scheme, firstly, a material to be detected with certain fineness is mixed with ethylenediamine tetraacetic acid and diethyl ether, so that an extraction system of a composite component is constructed, and the azo dye is fully dissolved out under the action of the extraction system; on the basis, the invention adopts a centrifugation and layering method to separate extraction phases, and further utilizes a low-temperature vacuum drying means to extract the component to be detected. In addition, the isoascorbic acid and 2-aminoindan hydrochloride are added before detection to play a role in protection, and a composite system to be detected is further constructed by utilizing the components of the ethyl oxalate, the dicarboxymethylalanine trisodium and the like. On the basis of the technical scheme, the invention performs detection through HPLC, and obtains a detection result by specific chromatographic conditions and an elution method. The invention has the advantages of simple operation, high detection speed, high accuracy, outstanding technical advantages and good popularization prospect.
Detailed Description
Hereinafter, specific embodiments of the present invention will be described in detail. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to identify quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
A method for rapidly detecting azo dyes in textiles comprises the following steps:
1) crushing the textile to be detected by using a homogenizer, mixing the crushed textile with ethylenediamine tetraacetic acid, uniformly mixing the crushed textile with the ethylenediamine tetraacetic acid, adding diethyl ether, mixing and centrifuging the mixture until the liquid is layered, and transferring the lower liquid phase into another container;
2) drying the other container in vacuum drying equipment, taking the residual solid phase, adding an isoascorbic acid aqueous solution into the residual solid phase, repeatedly blowing and absorbing until redissolving, adding dehydroabietylamine acetic acid, heating to 75 ℃, and keeping for 20 min;
3) adding the ethyl oxalate, the 3-methylphosphinic acid and the trisodium dicarboxymethylalanine into the product obtained in the step 2), performing vortex mixing assisted ultrasonic extraction, adding 2-aminoindan hydrochloride into the product, and filtering the product through a filter membrane with the aperture of 0.22 mu m to obtain a substance to be detected;
4) detecting the substance to be detected obtained in the step 3) under the following chromatographic conditions: the chromatographic column is a C18 column; the detector is VWD; the mobile phase A is methanol, and the mobile phase B is isooctane; gradient elution; in the first 8min of gradient elution, the volume fraction of methanol is reduced from 80% to 30%, and the volume fraction of isooctane is increased from 20% to 70%; and in the 8 th-20 th min of gradient elution, the volume fraction of methanol is increased from 30% to 80%, and the volume fraction of isooctane is decreased from 70% to 20%.
Example 2
A method for rapidly detecting azo dyes in textiles comprises the following steps:
1) crushing the textile to be detected by using a homogenizer, mixing the crushed textile with ethylenediamine tetraacetic acid, uniformly mixing the crushed textile with the ethylenediamine tetraacetic acid, adding diethyl ether, mixing and centrifuging the mixture until the liquid is layered, and transferring the lower liquid phase into another container;
2) drying the other container in vacuum drying equipment, taking the residual solid phase, adding an isoascorbic acid aqueous solution into the residual solid phase, repeatedly blowing and absorbing until redissolving, adding dehydroabietylamine acetic acid, heating to 75 ℃, and keeping for 20 min;
3) adding the ethyl oxalate, the 3-methylphosphinic acid and the trisodium dicarboxymethylalanine into the product obtained in the step 2), performing vortex mixing assisted ultrasonic extraction, adding 2-aminoindan hydrochloride into the product, and filtering the product through a filter membrane with the aperture of 0.22 mu m to obtain a substance to be detected;
4) detecting the substance to be detected obtained in the step 3) under the following chromatographic conditions: the chromatographic column is a C18 column; the detector is VWD; the mobile phase A is methanol, and the mobile phase B is isooctane; gradient elution; in the first 8min of gradient elution, the volume fraction of methanol is reduced from 80% to 30%, and the volume fraction of isooctane is increased from 20% to 70%; and in the 8 th-20 th min of gradient elution, the volume fraction of methanol is increased from 30% to 80%, and the volume fraction of isooctane is decreased from 70% to 20%.
Wherein, the particle size of the textile to be detected after the pulverization in the step 1) is not more than 1 mm. The molar ratio of the ethylene diamine tetraacetic acid to the diethyl ether in the step 1) is 1: 5. In step 1), the temperature does not exceed 8 ℃ during the transfer. The temperature of vacuum drying in the step 2) is not higher than 65 ℃, and the time of vacuum drying is not more than 40 min. The concentration of the isoascorbic acid aqueous solution in the step 2) is 0.8 mol/L. The final concentration of dehydroabietylamine acetic acid in the step 2) was 0.6 mol/L. The mol ratio of the ethyl ester of the methionine, the 3-methylphosphinic acid and the trisodium dicarboxymethylalanine in the step 3) is 1: 2: 3.6. The duration of the vortex mixing assisted ultrasonic extraction in the step 3) is 80-120 min. In step 3), the material to be filtered is heated to 55 ℃ before passing through a filter membrane with a pore diameter of 0.22 mu m.
The embodiments of the present invention have been described in detail, but the description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. Any modification, equivalent replacement, and improvement made within the scope of the application of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for rapidly detecting azo dyes in textiles is characterized by comprising the following steps:
1) crushing the textile to be detected by using a homogenizer, mixing the crushed textile with ethylenediamine tetraacetic acid, uniformly mixing the crushed textile with the ethylenediamine tetraacetic acid, adding diethyl ether, mixing and centrifuging the mixture until the liquid is layered, and transferring the lower liquid phase into another container;
2) drying the other container in vacuum drying equipment, taking the residual solid phase, adding an isoascorbic acid aqueous solution into the residual solid phase, repeatedly blowing and absorbing until redissolving, adding dehydroabietylamine acetic acid, heating to 75 ℃, and keeping for 20 min;
3) adding ethyl oxalate, 3-methylphosphinic acid and trisodium dicarboxymethylalanine into the product obtained in the step 2), performing vortex mixing assisted ultrasonic extraction, adding 2-aminoindane hydrochloride, and filtering with a 0.22-micrometer-aperture filter membrane to obtain a substance to be detected;
4) detecting the substance to be detected obtained in the step 3) under the following chromatographic conditions: the chromatographic column is a C18 column; the detector is VWD; the mobile phase A is methanol, and the mobile phase B is isooctane; gradient elution; in the first 8min of gradient elution, the volume fraction of methanol is reduced from 80% to 30%, and the volume fraction of isooctane is increased from 20% to 70%; and in the 8 th-20 th min of gradient elution, the volume fraction of methanol is increased from 30% to 80%, and the volume fraction of isooctane is decreased from 70% to 20%.
2. The method for rapidly detecting azo dyes in textiles according to claim 1, wherein the particle size of the textiles to be detected after the pulverization in step 1) is not more than 1 mm.
3. The method for rapidly detecting azo dyes in textiles as claimed in claim 1, wherein the molar ratio of ethylenediamine tetraacetic acid to diethyl ether in step 1) is 1: 5.
4. A method for rapid detection of azo dyes in textiles as claimed in claim 1, wherein in step 1), the temperature does not exceed 8 ℃ during said transfer.
5. The method for rapidly detecting azo dyes in textiles as claimed in claim 1, wherein the temperature for vacuum drying in step 2) is not higher than 65 ℃ and the time for vacuum drying is not more than 40 min.
6. The method for rapidly detecting azo dyes in textiles as claimed in claim 1, wherein the concentration of the aqueous solution of erythorbic acid in step 2) is 0.8 mol/L.
7. The method for rapidly detecting azo dyes in textiles according to claim 1, wherein the final concentration of dehydroabietylamine acetic acid in step 2) is 0.6 mol/L.
8. The method for rapidly detecting azo dyes in textiles as claimed in claim 1, wherein the molar ratio of ethyl ester of serine, 3-methylphosphonous acid propionic acid, and trisodium dicarboxymethylalanine in step 3) is 1: 2: 3.6.
9. The method for rapidly detecting the azo dye in the textile according to claim 1, wherein the time period of the vortex mixing assisted ultrasonic extraction in the step 3) is 80-120 min.
10. The method for rapidly detecting azo dyes in textiles as claimed in claim 1, wherein in step 3), the substance to be filtered is heated to 55 ℃ before passing through a 0.22 μm pore size filter.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210164635.XA CN114544832A (en) | 2022-02-22 | 2022-02-22 | Method for rapidly detecting azo dye in textile |
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| CN202210164635.XA CN114544832A (en) | 2022-02-22 | 2022-02-22 | Method for rapidly detecting azo dye in textile |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016035405A1 (en) * | 2014-09-02 | 2016-03-10 | 富士フイルム株式会社 | Azo dye composition and method for producing same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016035405A1 (en) * | 2014-09-02 | 2016-03-10 | 富士フイルム株式会社 | Azo dye composition and method for producing same |
Non-Patent Citations (2)
| Title |
|---|
| 贾永娟 等: "高效液相色谱法检测丙烯腈-丁二烯-苯乙烯塑料中多溴联苯醚" * |
| 黄伙水: "QuEChERS-超高效液相色谱-串联质谱法测定茶叶中氟唑磺隆和氟吡磺隆含量" * |
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